Phenol → HCID 58525342、化合物

HRID 1626358ノート

反応式

HRID 1626358 の反応式
Cl[C:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][N:5]=[C:4]([NH:12][C:13]2[CH:28]=[CH:27][C:16]([C:17]([NH:19][CH:20]3[CH2:25][CH2:24][N:23]([CH3:26])[CH2:22][CH2:21]3)=[O:18])=[CH:15][C:14]=2[O:29][CH3:30])[N:3]=1.[C:31]1([OH:37])[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1.N1C=CC=CC=1.C([O-])([O-])=O.[Cs+].[Cs+]>O1CCOCC1.CO>[CH3:30][O:29][C:14]1[CH:15]=[C:16]([CH:27]=[CH:28][C:13]=1[NH:12][C:4]1[N:3]=[C:2]([O:37][C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][N:5]=1)[C:17]([NH:19][CH:20]1[CH2:25][CH2:24][N:23]([CH3:26])[CH2:22][CH2:21]1)=[O:18]

参加物

7

反応物 4

HCID 996PhenolHCID 1049PyridineHCID 10796Cesium carbonateHCID 582009164-(4-chloro-5-trifluoromethyl-pyrimidin-2-ylamino)-3-methoxy-N-(1-methyl-piperidin-4-yl)-benzamide

生成物 1

HCID 58525342HCID 58525342、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
80 °C

実験手順

4-(4-chloro-5-trifluoromethyl-pyrimidin-2-ylamino)-3-methoxy-N-(1-methyl-piperidin-4-yl)-benzamide (50 mg) and phenol (21.3 mg) are dissolved in dioxane (0.3 mL). Pyridine (36.4 μL) and Cs2CO3 (235 mg) are added and the suspension is stirred overnight at 80° C. Then the reaction mixture is diluted with methanol (5 mL) and mixed with isolute. The solvent is eliminated in vacuo and then the mixture is purified by preparative HPLC. (PTK2 IC50=35 nmol)

後処理

  1. additionmixed with isolute
  2. customthe mixture is purified by preparative HPLC

出典と根拠

ORDレコード
ord-bbc8a45a5ada46bdb8e6b87c892f7dd5
出典データセット
uspto-grants-2014_07
特許番号
US08785464B2

反応ノート

読み込み中…